CN104628002B - A kind of method for preparation of active carbon based on catkin - Google Patents
A kind of method for preparation of active carbon based on catkin Download PDFInfo
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- CN104628002B CN104628002B CN201510062117.7A CN201510062117A CN104628002B CN 104628002 B CN104628002 B CN 104628002B CN 201510062117 A CN201510062117 A CN 201510062117A CN 104628002 B CN104628002 B CN 104628002B
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Abstract
A kind of method for preparation of active carbon based on catkin is by catkin：The g of absolute ethyl alcohol=10：300 900 ml, in absolute ethyl alcohol, then through filtering pure catkin is obtained by catkin by ultrasonic disperse；Under an inert atmosphere, carbonize, activation, by the activated carbon sample after activation successively through pickling and washing process, until filtrate clarification, pH reach 7；Again through 90 120oC drying process, is made activated carbon.The present invention, which has, utilizes natural catkin preparation duct prosperity, specific surface area high and nitrating activated carbon, both solves environmental problem, the advantage of huge economic benefit is produced again.
Description
Technical field
The invention belongs to a kind of preparation method of activated carbon, relate in particular to be prepared by a kind of activated carbon based on catkin
Method.
Background technology
The features such as activated carbon is with its good electrology characteristic, aboundresources, various structures and suitable price, it has also become most
Has the electrode material for super capacitor of commercial competitiveness.Activated carbon is general using carbon containing precursor as raw material, through high temperature carbonization, activation
Prepare.At present, preparing the presoma of activated carbon mainly has coal, oil, timber, polymer and biological material.Wherein,
Biomass is wide because of source, tool recyclability and its exquisite surfaces externally and internally and highly regular geometry, by increasingly
The attention of many researchers.
Catkin is as a kind of natural product of north of China, and when every spring and summer replaces, the catkin flown upward everywhere just gives people
Life bring many harm.For example, catkin incidentally propagates pollen during wafting, some allergic constitutions can be caused
The symptoms such as person's appearance is had a running nose, sneezed, being short of breath, pruitus, serious can also influence sleep；And catkin is very light,
Easily assemble agglomerating into fire " blasting fuse ".Therefore, catkin is effectively utilized has important meaning for resource, environment and social development
Justice.
Yanwei Ma et al. were reported using catkin as raw material first in 2011, passed through the method for direct carbonization
It is prepared for oxygen reduction electrode material (Carbon, 2011,49 (2): 573-580).But the method for this direct carbonization is profit
With catkin original pore passage structure and surface chemical property, lack the artificial regulatory to target material pore passage structure, compare surface
Small, only 257 m of product2/g。
The content of the invention
It is an object of the invention to provide a kind of method for preparation of active carbon based on catkin, duct is prepared using natural catkin
The activated carbon of flourishing, specific surface area height and nitrating, both solves environmental problem, huge economic benefit is produced again.
The technical proposal for solving the technical problem of the invention is：
The present invention sequentially passes through the processing steps such as pretreatment, charing, activation, post processing, finally using natural catkin as raw material
Obtain active carbon electrode material for super capacitor.
The characteristics of the inventive method lies also in be operated as follows：
(1) pre-process：Press catkin：The g of absolute ethyl alcohol=10：300-900 ml, by catkin by ultrasonic disperse in anhydrous second
In alcohol, then through the pure catkin of filtering acquisition；
(2) carbonize：In inertia（Nitrogen or argon gas）Under atmosphere, pretreated catkin is placed in retort, in 400-
1000 oAt a temperature of C, 1-3 h are carbonized；
(3) activate：Catkin after charing and potassium hydroxide are pressed 1:The ethanol that 1-4 mass ratioes are dispersed in 50 wt% is water-soluble
In liquid, then drying processing, it is subsequently placed in activation furnace, in inertia（Nitrogen or argon gas）Under atmosphere, in 600-800oIt is permanent under C
Warm 20-70 min, then naturally cool to room temperature, obtain activated carbon sample；
(4) post-process：By the activated carbon sample after activation successively through pickling and washing process, until filtrate clarification, pH reach
To 7；Again through 90-120oC drying process, is made activated carbon.
The specific surface area that the present invention prepares activated carbon reaches 1000-2500 m2/G, nitrogen content is 1wt%-5wt%.
The present invention has the advantages that compared with prior art：
（1）The present invention use catkin for raw material, and cost is low, and solves environmental problem and generate huge economy again and imitate
Benefit.
（2）The present invention makes full use of the pore passage structure of catkin itself and itself is nitrogenous, after the processing such as charing, activation
Institute's preparing active carbon has hierarchical porous structure, and specific surface area is big, high nitrogen content, while larger specific capacitance is provided, keeps higher
High rate performance, be preferable electrode for super capacitor material.
（3）Step of the present invention is simple, and easy to operate, energy consumption is low, and capacitance characteristic is good, with good application prospect.
Brief description of the drawings
The electromicroscopic photograph of the product of Fig. 1 embodiments 4.
The product of Fig. 2 embodiments 4 is in the different cyclic voltammetry curves swept under speed.
Embodiment
The present invention is further illustrated with embodiment below, but protection scope of the present invention is not limited in embodiment.It is right
The other changes and modifications that those skilled in the art makes in the case of the spirit and scope without departing substantially from the present invention, still
It is included within the scope of the present invention.
Embodiment 1
10 g catkins in 300 ml ethanol solutions, then through filtering are obtained into pure catkin by ultrasonic disperse；
The catkin of wetting is placed in retort successively, under argon atmosphere, 400oAt a temperature of C, 3 h are carbonized, carbonized material is obtained；
Then the catkin after charing and potassium hydroxide are pressed 1:1 mass ratio is dispersed in 50 wt% ethanol water, then at drying
Reason, is subsequently placed in activation furnace, under nitrogen atmosphere, 800oThe min of constant temperature 20, naturally cools to room temperature under C, is lived
Property charcoal sample；Finally by the activated carbon sample after activation successively through pickling and washing process, until filtrate clarification, pH reach 7；Again
Through 90oC drying process, preparation specific surface area is 1020 m2/ g, nitrogen content is 3.12wt% activated carbon.
According to mass ratio 85:10:5 ratio adds obtained activated carbon, acetylene black, polytetrafluoroethylene (PTFE), and mixing is rolled into
A diameter of 1 cm is struck out after film2Electrode slice, using 6 M KOH as electrolyte, current density be 1 A/g when, it is than electricity
Capacity is 158 F/g.
Embodiment 2
10 g catkins in 600 ml ethanol solutions, then through filtering are obtained into pure catkin by ultrasonic disperse；
The catkin of wetting is placed in retort successively, under nitrogen atmosphere, 500oAt a temperature of C, 1.5 h are carbonized, are carbonized
Material；Then the catkin after charing and potassium hydroxide are pressed 1:3 mass ratioes are dispersed in 50 wt% ethanol water, then drying
Processing, is subsequently placed in activation furnace, under nitrogen atmosphere, 600oThe min of constant temperature 50 under C, naturally cools to room temperature, obtains
Activated carbon sample；Finally by the activated carbon sample after activation successively through pickling and washing process, until filtrate clarification, pH reach 7；
Again through 120oC drying process, preparation specific surface area is 1340m2/ g, nitrogen content is 4.92wt% activated carbon.
Identical with the method that embodiment 1 prepares electrode, after tested, when current density is 1 A/g, its specific capacitance is
172 F/g。
Embodiment 3
10 g catkins in 900 ml ethanol solutions, then through filtering are obtained into pure catkin by ultrasonic disperse；
The catkin of wetting is placed in retort successively, under argon atmosphere, 1000oAt a temperature of C, 1 h is carbonized, carbonized material is obtained；
Then the catkin after charing and potassium hydroxide are pressed 1:4 mass ratioes are dispersed in 50 wt% ethanol water, then at drying
Reason, is subsequently placed in activation furnace, under argon atmosphere, 600oThe min of constant temperature 70, naturally cools to room temperature under C, is lived
Property charcoal sample；Finally by the activated carbon sample after activation successively through pickling and washing process, until filtrate clarification, pH reach 7；Again
Through 105oC drying process, preparation specific surface area is 1540 m2/ g, nitrogen content is 2.56 wt% activated carbon.
Identical with the method that embodiment 1 prepares electrode, after tested, when current density is 1 A/g, its specific capacitance is
185 F/g。
Embodiment 4
10 g catkins in 900 ml ethanol solutions, then through filtering are obtained into pure catkin by ultrasonic disperse；
The catkin of wetting is placed in retort successively, under argon atmosphere, 500oAt a temperature of C, 1 h is carbonized, carbonized material is obtained；
Then the catkin after charing and potassium hydroxide are pressed 1:4 mass ratioes are dispersed in 50 wt% ethanol water, then at drying
Reason, is subsequently placed in activation furnace, under argon atmosphere, 800oThe min of constant temperature 60, naturally cools to room temperature under C, is lived
Property charcoal sample；Finally by the activated carbon sample after activation successively through pickling and washing process, until filtrate clarification, pH reach 7；Again
Through 105oC drying process, preparation specific surface area is 2300 m2/ g, nitrogen content is 3.42 wt% activated carbon.
Identical with the method that embodiment 1 prepares electrode, after tested, when current density is 1 A/g, its specific capacitance is
303F/g。
Embodiment 5
10 g catkins in 800 ml ethanol solutions, then through filtering are obtained into pure catkin by ultrasonic disperse；
The catkin of wetting is placed in retort successively, under nitrogen atmosphere, 700oAt a temperature of C, 1 h is carbonized, carbonized material is obtained；
Then the catkin after charing and potassium hydroxide are pressed 1:2 mass ratioes are dispersed in 50 wt% ethanol water, then at drying
Reason, is subsequently placed in activation furnace, under nitrogen atmosphere, 800oThe min of constant temperature 60, naturally cools to room temperature under C, is lived
Property charcoal sample；Finally by the activated carbon sample after activation successively through pickling and washing process, until filtrate clarification, pH reach 7；Again
Through 100oC drying process, preparation specific surface area is 1120 m2/ g, nitrogen content is 2.12 wt% activated carbon.
Identical with the method that embodiment 1 prepares electrode, after tested, when current density is 1A/g, its specific capacitance is 170
F/g。
Embodiment 6
Catkin in ethanol solution, then through filtering is obtained into pure catkin by ultrasonic disperse；Successively will wetting
Catkin be placed in retort, under argon atmosphere, 1000oAt a temperature of C, 1 h is carbonized, carbonized material is obtained；Then will charing
Catkin afterwards presses 1 with potassium hydroxide:4 mass ratioes are dispersed in 50wt% ethanol water, then drying processing, are subsequently placed in
In activation furnace, under nitrogen atmosphere, 800oThe min of constant temperature 60 under C, naturally cools to room temperature, obtains activated carbon sample；Finally
By the activated carbon sample after activation successively through pickling and washing process, until filtrate clarification, pH reach 7；Again through 105oAt C dryings
Reason, preparation specific surface area is 1670m2/ g, nitrogen content is 1.14 wt% activated carbon.
Identical with the method that embodiment 1 prepares electrode, after tested, when current density is 1A/g, its specific capacitance is 220
F/g。
Claims (2)
1. a kind of method for preparation of active carbon based on catkin, it is characterised in that comprise the following steps：
(1) pre-process：Press catkin：The g of absolute ethyl alcohol=10：300-900 ml, by catkin by ultrasonic disperse in absolute ethyl alcohol
In, then through the pure catkin of filtering acquisition；
(2) carbonize：Under an inert atmosphere, pretreated catkin is placed in retort, in 400-1000oAt a temperature of C, charing
1-3 h；
(3) activate：Catkin after charing and potassium hydroxide are pressed 1:1-4 mass ratioes are dispersed in 50 wt% ethanol water,
Drying is handled again, is subsequently placed in activation furnace, under an inert atmosphere, in 600-800oConstant temperature 20-70 min under C, then
Room temperature is naturally cooled to, activated carbon sample is obtained；
(4) post-process：By the activated carbon sample after activation successively through pickling and washing process, until filtrate clarification, pH reach 7；
Again through 90-120oC drying process, is made activated carbon；
The specific surface area for preparing activated carbon reaches 1000-2500m2/ g, nitrogen content is 1wt%-5wt%.
2. a kind of method for preparation of active carbon based on catkin as claimed in claim 1, it is characterised in that described inert atmosphere
For nitrogen or argon gas.
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| CN106185922A (en) * | 2016-07-06 | 2016-12-07 | 江苏大学 | The preparation method and its usage of one level hole, Yeasts Quito material with carbon element |
| CN107903575B (en) * | 2017-10-18 | 2020-05-01 | 中国科学院山西煤炭化学研究所 | Preparation method of graphene phenolic resin-based composite fiber film for capacitor electrode |
| CN108821284B (en) * | 2018-09-08 | 2020-01-31 | 张小泉 | Preparation method of Artemisia desertorum biochar |
| CN111892050A (en) * | 2020-09-01 | 2020-11-06 | 杨正 | Preparation method for producing layered porous activated carbon with high specific surface area |
| CN113926439A (en) * | 2021-11-10 | 2022-01-14 | 河海大学 | Method for preparing phosphorus removal adsorbent based on phoenix tree batting |
| CN114316922B (en) * | 2022-01-13 | 2023-08-22 | 郑州大学 | Composite phase change material for packaging lauric acid and preparation method thereof |
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